# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_dvg-69 _database_code_CSD 177246 _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Vila, Jose M.' 'Castro-Juiz, Samuel' 'Fernandez, Alberto' 'Fernandez, Jesus J.' 'Lopez-Torres, Margarita' 'Suarez, Antonio' 'Vazquez-Garcia, Digna' _publ_contact_author_name 'Dr Jose M. Vila' _publ_contact_author_address ; Inorganic Chemistry University of Santiago Facultad de Química, Av. de las Cie Santiago de Compostela 15782 SPAIN ; _publ_contact_author_email 'QIDEPORT@USC.ES' _publ_section_title ; Synthesis and Reactivity of Novel Tetranuclear Cyclometallated Complexes Derived From [C,N,O] Terdentate Ligands. Crystal Structure of [Pd{2,3,4-(MeO)3C6HC(H)=N[2-(O)C6H4]}(PPh3)] ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 N O4 P Pd' _chemical_formula_weight 653.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.4084(13) _cell_length_b 12.0132(5) _cell_length_c 18.3250(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.171(8) _cell_angle_gamma 90.00 _cell_volume 5875.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7130 _exptl_absorpt_correction_T_max 0.8685 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% < 0 _diffrn_reflns_number 20437 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7230 _reflns_number_gt 4859 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+2.3709P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7230 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.122593(8) 0.019121(19) 0.136067(12) 0.03775(8) Uani 1 1 d . . . P1 P 0.16908(3) -0.09040(6) 0.07772(4) 0.03666(18) Uani 1 1 d . . . O1 O 0.11753(10) -0.3680(2) 0.30121(15) 0.0703(7) Uani 1 1 d . . . O2 O 0.06573(10) -0.2646(2) 0.38791(13) 0.0714(7) Uani 1 1 d . . . O3 O 0.03941(16) -0.0331(3) 0.35707(19) 0.1178(14) Uani 1 1 d . . . O4 O 0.12452(9) 0.16444(18) 0.07330(12) 0.0544(6) Uani 1 1 d . . . N1 N 0.08403(9) 0.1211(2) 0.18950(14) 0.0435(6) Uani 1 1 d . . . C1 C 0.10873(11) -0.0905(2) 0.21253(16) 0.0414(7) Uani 1 1 d . . . C3 C 0.10586(12) -0.2581(3) 0.28413(18) 0.0491(8) Uani 1 1 d . . . C2 C 0.12062(12) -0.2013(3) 0.22638(17) 0.0474(8) Uani 1 1 d . . . H2 H 0.1387 -0.2387 0.1968 0.057 Uiso 1 1 calc R . . C4 C 0.07793(13) -0.2067(3) 0.32915(17) 0.0523(8) Uani 1 1 d . . . C5 C 0.06563(13) -0.0948(3) 0.31741(18) 0.0561(9) Uani 1 1 d . . . C6 C 0.08096(12) -0.0373(3) 0.25966(18) 0.0483(8) Uani 1 1 d . . . C7 C 0.06927(13) 0.0790(3) 0.24481(18) 0.0538(8) Uani 1 1 d . . . H7 H 0.0521 0.1206 0.2737 0.065 Uiso 1 1 calc R . . C8 C 0.07970(11) 0.2315(3) 0.16202(17) 0.0456(7) Uani 1 1 d . . . C9 C 0.05778(13) 0.3195(3) 0.1928(2) 0.0568(9) Uani 1 1 d . . . H9 H 0.0444 0.3078 0.2344 0.068 Uiso 1 1 calc R . . C10 C 0.05620(15) 0.4233(3) 0.1611(2) 0.0705(11) Uani 1 1 d . . . H10 H 0.0423 0.4829 0.1817 0.085 Uiso 1 1 calc R . . C11 C 0.07550(15) 0.4386(3) 0.0980(2) 0.0721(11) Uani 1 1 d . . . H11 H 0.0734 0.5085 0.0756 0.087 Uiso 1 1 calc R . . C12 C 0.09764(14) 0.3530(3) 0.0677(2) 0.0628(10) Uani 1 1 d . . . H12 H 0.1103 0.3659 0.0256 0.075 Uiso 1 1 calc R . . C13 C 0.10131(12) 0.2464(3) 0.09954(18) 0.0477(8) Uani 1 1 d . . . C14 C 0.15538(16) -0.4181(3) 0.2711(2) 0.0786(12) Uani 1 1 d . . . H14A H 0.1597 -0.4942 0.2873 0.118 Uiso 1 1 calc R . . H14B H 0.1863 -0.3786 0.2881 0.118 Uiso 1 1 calc R . . H14C H 0.1458 -0.4157 0.2173 0.118 Uiso 1 1 calc R . . C15 C 0.02474(19) -0.3374(4) 0.3666(3) 0.1028(17) Uani 1 1 d . . . H15A H 0.0186 -0.3739 0.4102 0.154 Uiso 1 1 calc R . . H15B H 0.0321 -0.3920 0.3324 0.154 Uiso 1 1 calc R . . H15C H -0.0044 -0.2959 0.3425 0.154 Uiso 1 1 calc R . . C16 C 0.02694(18) -0.0567(4) 0.4205(2) 0.0947(15) Uani 1 1 d . . . H16A H 0.0081 0.0040 0.4344 0.142 Uiso 1 1 calc R . . H16B H 0.0567 -0.0684 0.4591 0.142 Uiso 1 1 calc R . . H16C H 0.0069 -0.1230 0.4144 0.142 Uiso 1 1 calc R . . C17 C 0.21394(11) -0.1805(2) 0.13902(16) 0.0405(7) Uani 1 1 d . . . C18 C 0.22300(13) -0.2900(3) 0.12143(19) 0.0527(8) Uani 1 1 d . . . H18 H 0.2048 -0.3212 0.0771 0.063 Uiso 1 1 calc R . . C19 C 0.25903(15) -0.3533(3) 0.1697(2) 0.0692(11) Uani 1 1 d . . . H19 H 0.2650 -0.4264 0.1575 0.083 Uiso 1 1 calc R . . C20 C 0.28568(14) -0.3078(4) 0.2351(2) 0.0728(12) Uani 1 1 d . . . H20 H 0.3097 -0.3503 0.2673 0.087 Uiso 1 1 calc R . . C21 C 0.27721(14) -0.1989(4) 0.2538(2) 0.0690(11) Uani 1 1 d . . . H21 H 0.2958 -0.1681 0.2980 0.083 Uiso 1 1 calc R . . C22 C 0.24096(12) -0.1363(3) 0.20634(18) 0.0541(8) Uani 1 1 d . . . H22 H 0.2346 -0.0639 0.2196 0.065 Uiso 1 1 calc R . . C23 C 0.20801(11) -0.0101(2) 0.02803(16) 0.0404(7) Uani 1 1 d . . . C24 C 0.25973(13) -0.0164(3) 0.0459(2) 0.0594(9) Uani 1 1 d . . . H24 H 0.2757 -0.0661 0.0826 0.071 Uiso 1 1 calc R . . C25 C 0.28799(14) 0.0501(4) 0.0101(2) 0.0770(12) Uani 1 1 d . . . H25 H 0.3228 0.0450 0.0229 0.092 Uiso 1 1 calc R . . C26 C 0.26538(16) 0.1238(3) -0.0445(2) 0.0700(11) Uani 1 1 d . . . H26 H 0.2846 0.1699 -0.0676 0.084 Uiso 1 1 calc R . . C27 C 0.21369(16) 0.1285(3) -0.0644(2) 0.0665(10) Uani 1 1 d . . . H27 H 0.1980 0.1758 -0.1027 0.080 Uiso 1 1 calc R . . C28 C 0.18517(13) 0.0637(3) -0.02802(19) 0.0562(9) Uani 1 1 d . . . H28 H 0.1504 0.0693 -0.0410 0.067 Uiso 1 1 calc R . . C29 C 0.13242(11) -0.1824(2) 0.00696(16) 0.0409(7) Uani 1 1 d . . . C30 C 0.08640(13) -0.2197(3) 0.01529(18) 0.0548(9) Uani 1 1 d . . . H30 H 0.0741 -0.1958 0.0559 0.066 Uiso 1 1 calc R . . C31 C 0.05816(15) -0.2932(3) -0.0370(2) 0.0714(11) Uani 1 1 d . . . H31 H 0.0270 -0.3175 -0.0316 0.086 Uiso 1 1 calc R . . C32 C 0.07696(16) -0.3289(3) -0.0960(2) 0.0688(11) Uani 1 1 d . . . H32 H 0.0587 -0.3791 -0.1302 0.083 Uiso 1 1 calc R . . C33 C 0.12215(15) -0.2917(3) -0.1053(2) 0.0690(11) Uani 1 1 d . . . H33 H 0.1342 -0.3160 -0.1461 0.083 Uiso 1 1 calc R . . C34 C 0.15022(13) -0.2178(3) -0.05447(18) 0.0554(9) Uani 1 1 d . . . H34 H 0.1808 -0.1920 -0.0614 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03732(13) 0.04091(13) 0.03717(12) -0.00050(10) 0.01298(9) 0.00225(11) P1 0.0358(4) 0.0411(4) 0.0346(4) -0.0008(3) 0.0111(3) 0.0020(3) O1 0.0826(19) 0.0549(16) 0.0817(18) 0.0164(13) 0.0360(15) -0.0004(13) O2 0.0881(19) 0.0801(18) 0.0519(14) 0.0099(13) 0.0285(14) -0.0197(15) O3 0.184(4) 0.103(2) 0.104(2) 0.0288(19) 0.111(3) 0.047(2) O4 0.0670(16) 0.0485(13) 0.0551(14) 0.0096(10) 0.0296(12) 0.0131(11) N1 0.0397(15) 0.0478(15) 0.0437(14) -0.0033(12) 0.0108(12) 0.0042(12) C1 0.0409(17) 0.0449(18) 0.0400(15) -0.0006(13) 0.0127(13) -0.0036(13) C3 0.0501(19) 0.0466(19) 0.0522(19) 0.0042(15) 0.0149(16) -0.0072(15) C2 0.0488(19) 0.050(2) 0.0478(18) -0.0018(15) 0.0197(15) -0.0033(15) C4 0.053(2) 0.066(2) 0.0401(17) 0.0076(16) 0.0140(16) -0.0122(17) C5 0.058(2) 0.069(2) 0.0484(19) 0.0026(17) 0.0277(17) 0.0009(18) C6 0.0488(19) 0.055(2) 0.0450(17) 0.0032(15) 0.0186(15) 0.0021(15) C7 0.057(2) 0.061(2) 0.0500(19) -0.0039(17) 0.0248(17) 0.0092(17) C8 0.0379(17) 0.0485(19) 0.0481(18) -0.0029(14) 0.0053(14) 0.0063(14) C9 0.052(2) 0.060(2) 0.059(2) -0.0059(17) 0.0139(17) 0.0126(17) C10 0.073(3) 0.052(2) 0.082(3) -0.009(2) 0.009(2) 0.021(2) C11 0.076(3) 0.047(2) 0.088(3) 0.008(2) 0.009(2) 0.008(2) C12 0.064(2) 0.056(2) 0.069(2) 0.0115(18) 0.017(2) 0.0057(19) C13 0.0421(18) 0.0486(19) 0.0505(18) 0.0052(15) 0.0067(15) 0.0053(15) C14 0.082(3) 0.057(2) 0.102(3) 0.022(2) 0.031(3) 0.014(2) C15 0.127(4) 0.110(4) 0.083(3) -0.003(3) 0.050(3) -0.060(3) C16 0.100(4) 0.134(4) 0.063(3) 0.005(3) 0.045(3) 0.025(3) C17 0.0351(16) 0.0487(18) 0.0394(16) 0.0033(13) 0.0119(13) 0.0026(13) C18 0.057(2) 0.051(2) 0.0504(19) 0.0023(16) 0.0139(17) 0.0061(16) C19 0.071(3) 0.058(2) 0.082(3) 0.018(2) 0.027(2) 0.023(2) C20 0.047(2) 0.091(3) 0.078(3) 0.040(2) 0.009(2) 0.017(2) C21 0.051(2) 0.100(3) 0.050(2) 0.012(2) -0.0005(18) -0.007(2) C22 0.051(2) 0.064(2) 0.0456(18) 0.0029(16) 0.0094(16) 0.0022(17) C23 0.0418(17) 0.0430(17) 0.0398(15) -0.0027(13) 0.0164(13) -0.0003(13) C24 0.047(2) 0.075(2) 0.057(2) 0.0169(18) 0.0125(17) -0.0025(18) C25 0.042(2) 0.107(3) 0.084(3) 0.019(3) 0.019(2) -0.015(2) C26 0.079(3) 0.071(3) 0.067(2) 0.006(2) 0.034(2) -0.017(2) C27 0.081(3) 0.062(2) 0.061(2) 0.0214(18) 0.027(2) 0.008(2) C28 0.049(2) 0.065(2) 0.056(2) 0.0131(18) 0.0163(17) 0.0076(17) C29 0.0396(17) 0.0441(17) 0.0379(16) 0.0006(13) 0.0064(13) 0.0017(13) C30 0.053(2) 0.068(2) 0.0447(18) -0.0017(16) 0.0146(16) -0.0139(17) C31 0.063(2) 0.086(3) 0.062(2) 0.000(2) 0.008(2) -0.035(2) C32 0.082(3) 0.068(3) 0.050(2) -0.0111(18) 0.002(2) -0.019(2) C33 0.071(3) 0.081(3) 0.052(2) -0.023(2) 0.010(2) 0.006(2) C34 0.0449(19) 0.071(2) 0.052(2) -0.0131(17) 0.0143(16) -0.0021(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.012(2) . ? Pd1 C1 2.021(3) . ? Pd1 O4 2.098(2) . ? Pd1 P1 2.2624(8) . ? P1 C17 1.821(3) . ? P1 C29 1.822(3) . ? P1 C23 1.828(3) . ? O1 C3 1.377(4) . ? O1 C14 1.416(5) . ? O2 C4 1.385(4) . ? O2 C15 1.407(5) . ? O3 C16 1.316(5) . ? O3 C5 1.354(4) . ? O4 C13 1.321(4) . ? N1 C7 1.278(4) . ? N1 C8 1.414(4) . ? C1 C2 1.381(4) . ? C1 C6 1.426(4) . ? C3 C4 1.391(5) . ? C3 C2 1.395(4) . ? C4 C5 1.391(5) . ? C5 C6 1.406(4) . ? C6 C7 1.446(5) . ? C8 C9 1.396(4) . ? C8 C13 1.415(4) . ? C9 C10 1.372(5) . ? C10 C11 1.390(6) . ? C11 C12 1.373(5) . ? C12 C13 1.401(5) . ? C17 C18 1.390(4) . ? C17 C22 1.391(4) . ? C18 C19 1.392(5) . ? C19 C20 1.368(5) . ? C20 C21 1.384(6) . ? C21 C22 1.384(5) . ? C23 C24 1.382(4) . ? C23 C28 1.393(4) . ? C24 C25 1.379(5) . ? C25 C26 1.372(5) . ? C26 C27 1.381(5) . ? C27 C28 1.377(5) . ? C29 C30 1.379(4) . ? C29 C34 1.391(4) . ? C30 C31 1.399(5) . ? C31 C32 1.369(5) . ? C32 C33 1.364(5) . ? C33 C34 1.386(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 C1 81.75(11) . . ? N1 Pd1 O4 80.90(9) . . ? C1 Pd1 O4 162.65(10) . . ? N1 Pd1 P1 177.35(7) . . ? C1 Pd1 P1 99.44(9) . . ? O4 Pd1 P1 97.91(6) . . ? C17 P1 C29 105.29(14) . . ? C17 P1 C23 103.43(14) . . ? C29 P1 C23 104.81(14) . . ? C17 P1 Pd1 115.33(10) . . ? C29 P1 Pd1 114.24(10) . . ? C23 P1 Pd1 112.59(10) . . ? C3 O1 C14 118.2(3) . . ? C4 O2 C15 114.5(3) . . ? C16 O3 C5 129.3(4) . . ? C13 O4 Pd1 110.3(2) . . ? C7 N1 C8 129.6(3) . . ? C7 N1 Pd1 116.2(2) . . ? C8 N1 Pd1 114.1(2) . . ? C2 C1 C6 117.2(3) . . ? C2 C1 Pd1 133.0(2) . . ? C6 C1 Pd1 109.8(2) . . ? O1 C3 C4 114.9(3) . . ? O1 C3 C2 123.3(3) . . ? C4 C3 C2 121.8(3) . . ? C1 C2 C3 120.9(3) . . ? O2 C4 C3 120.1(3) . . ? O2 C4 C5 120.8(3) . . ? C3 C4 C5 119.0(3) . . ? O3 C5 C4 125.9(3) . . ? O3 C5 C6 114.9(3) . . ? C4 C5 C6 119.2(3) . . ? C5 C6 C1 121.9(3) . . ? C5 C6 C7 121.7(3) . . ? C1 C6 C7 116.4(3) . . ? N1 C7 C6 115.8(3) . . ? C9 C8 C13 121.9(3) . . ? C9 C8 N1 125.1(3) . . ? C13 C8 N1 113.0(3) . . ? C10 C9 C8 119.5(4) . . ? C9 C10 C11 119.4(4) . . ? C12 C11 C10 121.6(4) . . ? C11 C12 C13 120.9(4) . . ? O4 C13 C12 121.7(3) . . ? O4 C13 C8 121.7(3) . . ? C12 C13 C8 116.7(3) . . ? C18 C17 C22 118.6(3) . . ? C18 C17 P1 123.4(2) . . ? C22 C17 P1 117.9(2) . . ? C17 C18 C19 120.5(3) . . ? C20 C19 C18 119.9(4) . . ? C19 C20 C21 120.5(3) . . ? C20 C21 C22 119.7(4) . . ? C21 C22 C17 120.7(3) . . ? C24 C23 C28 118.3(3) . . ? C24 C23 P1 122.4(2) . . ? C28 C23 P1 119.2(2) . . ? C25 C24 C23 120.8(3) . . ? C26 C25 C24 120.7(4) . . ? C25 C26 C27 119.0(3) . . ? C28 C27 C26 120.7(3) . . ? C27 C28 C23 120.5(3) . . ? C30 C29 C34 119.2(3) . . ? C30 C29 P1 119.2(2) . . ? C34 C29 P1 121.5(2) . . ? C29 C30 C31 120.4(3) . . ? C32 C31 C30 119.3(4) . . ? C33 C32 C31 120.8(3) . . ? C32 C33 C34 120.4(4) . . ? C33 C34 C29 119.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 P1 C17 76.1(16) . . . . ? C1 Pd1 P1 C17 -40.51(14) . . . . ? O4 Pd1 P1 C17 139.05(13) . . . . ? N1 Pd1 P1 C29 -161.7(16) . . . . ? C1 Pd1 P1 C29 81.71(13) . . . . ? O4 Pd1 P1 C29 -98.73(12) . . . . ? N1 Pd1 P1 C23 -42.3(16) . . . . ? C1 Pd1 P1 C23 -158.88(14) . . . . ? O4 Pd1 P1 C23 20.67(13) . . . . ? N1 Pd1 O4 C13 0.9(2) . . . . ? C1 Pd1 O4 C13 1.8(5) . . . . ? P1 Pd1 O4 C13 -176.7(2) . . . . ? C1 Pd1 N1 C7 1.3(2) . . . . ? O4 Pd1 N1 C7 -179.0(2) . . . . ? P1 Pd1 N1 C7 -115.7(16) . . . . ? C1 Pd1 N1 C8 178.1(2) . . . . ? O4 Pd1 N1 C8 -2.2(2) . . . . ? P1 Pd1 N1 C8 61.1(17) . . . . ? N1 Pd1 C1 C2 179.6(3) . . . . ? O4 Pd1 C1 C2 178.7(3) . . . . ? P1 Pd1 C1 C2 -2.7(3) . . . . ? N1 Pd1 C1 C6 -0.3(2) . . . . ? O4 Pd1 C1 C6 -1.2(5) . . . . ? P1 Pd1 C1 C6 177.3(2) . . . . ? C14 O1 C3 C4 -165.0(3) . . . . ? C14 O1 C3 C2 15.0(5) . . . . ? C6 C1 C2 C3 0.1(5) . . . . ? Pd1 C1 C2 C3 -179.8(2) . . . . ? O1 C3 C2 C1 -178.7(3) . . . . ? C4 C3 C2 C1 1.2(5) . . . . ? C15 O2 C4 C3 -80.0(5) . . . . ? C15 O2 C4 C5 104.5(4) . . . . ? O1 C3 C4 O2 2.6(5) . . . . ? C2 C3 C4 O2 -177.4(3) . . . . ? O1 C3 C4 C5 178.2(3) . . . . ? C2 C3 C4 C5 -1.8(5) . . . . ? C16 O3 C5 C4 12.0(8) . . . . ? C16 O3 C5 C6 -168.1(5) . . . . ? O2 C4 C5 O3 -3.5(6) . . . . ? C3 C4 C5 O3 -179.0(4) . . . . ? O2 C4 C5 C6 176.6(3) . . . . ? C3 C4 C5 C6 1.1(5) . . . . ? O3 C5 C6 C1 -179.7(3) . . . . ? C4 C5 C6 C1 0.1(5) . . . . ? O3 C5 C6 C7 0.1(5) . . . . ? C4 C5 C6 C7 180.0(3) . . . . ? C2 C1 C6 C5 -0.7(5) . . . . ? Pd1 C1 C6 C5 179.2(3) . . . . ? C2 C1 C6 C7 179.4(3) . . . . ? Pd1 C1 C6 C7 -0.7(4) . . . . ? C8 N1 C7 C6 -178.2(3) . . . . ? Pd1 N1 C7 C6 -2.0(4) . . . . ? C5 C6 C7 N1 -178.1(3) . . . . ? C1 C6 C7 N1 1.8(4) . . . . ? C7 N1 C8 C9 0.8(5) . . . . ? Pd1 N1 C8 C9 -175.4(3) . . . . ? C7 N1 C8 C13 179.4(3) . . . . ? Pd1 N1 C8 C13 3.1(3) . . . . ? C13 C8 C9 C10 1.2(5) . . . . ? N1 C8 C9 C10 179.5(3) . . . . ? C8 C9 C10 C11 1.4(6) . . . . ? C9 C10 C11 C12 -2.1(6) . . . . ? C10 C11 C12 C13 0.3(6) . . . . ? Pd1 O4 C13 C12 179.5(3) . . . . ? Pd1 O4 C13 C8 0.6(4) . . . . ? C11 C12 C13 O4 -176.8(3) . . . . ? C11 C12 C13 C8 2.1(5) . . . . ? C9 C8 C13 O4 176.1(3) . . . . ? N1 C8 C13 O4 -2.5(4) . . . . ? C9 C8 C13 C12 -2.9(5) . . . . ? N1 C8 C13 C12 178.6(3) . . . . ? C29 P1 C17 C18 12.6(3) . . . . ? C23 P1 C17 C18 -97.1(3) . . . . ? Pd1 P1 C17 C18 139.5(2) . . . . ? C29 P1 C17 C22 -168.4(3) . . . . ? C23 P1 C17 C22 81.9(3) . . . . ? Pd1 P1 C17 C22 -41.5(3) . . . . ? C22 C17 C18 C19 -1.1(5) . . . . ? P1 C17 C18 C19 177.8(3) . . . . ? C17 C18 C19 C20 0.3(6) . . . . ? C18 C19 C20 C21 -0.2(6) . . . . ? C19 C20 C21 C22 1.0(6) . . . . ? C20 C21 C22 C17 -1.9(6) . . . . ? C18 C17 C22 C21 2.0(5) . . . . ? P1 C17 C22 C21 -177.1(3) . . . . ? C17 P1 C23 C24 -6.7(3) . . . . ? C29 P1 C23 C24 -116.8(3) . . . . ? Pd1 P1 C23 C24 118.4(3) . . . . ? C17 P1 C23 C28 175.9(3) . . . . ? C29 P1 C23 C28 65.8(3) . . . . ? Pd1 P1 C23 C28 -58.9(3) . . . . ? C28 C23 C24 C25 1.1(5) . . . . ? P1 C23 C24 C25 -176.3(3) . . . . ? C23 C24 C25 C26 -0.2(7) . . . . ? C24 C25 C26 C27 -1.7(7) . . . . ? C25 C26 C27 C28 2.7(6) . . . . ? C26 C27 C28 C23 -1.9(6) . . . . ? C24 C23 C28 C27 0.0(5) . . . . ? P1 C23 C28 C27 177.5(3) . . . . ? C17 P1 C29 C30 97.9(3) . . . . ? C23 P1 C29 C30 -153.3(3) . . . . ? Pd1 P1 C29 C30 -29.6(3) . . . . ? C17 P1 C29 C34 -80.8(3) . . . . ? C23 P1 C29 C34 28.0(3) . . . . ? Pd1 P1 C29 C34 151.7(2) . . . . ? C34 C29 C30 C31 0.7(5) . . . . ? P1 C29 C30 C31 -178.0(3) . . . . ? C29 C30 C31 C32 0.8(6) . . . . ? C30 C31 C32 C33 -1.6(6) . . . . ? C31 C32 C33 C34 0.8(6) . . . . ? C32 C33 C34 C29 0.8(6) . . . . ? C30 C29 C34 C33 -1.5(5) . . . . ? P1 C29 C34 C33 177.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.439 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.068